Decoding The Holy Grail: Terpene & Cannabinoid Retention: Decarb to Extraction

greatwolf said:
I'm hesitant to write this reply here but have decided to do so after some thought.

Some vendors, having the same problems you describe, are using MCT as the vape carrier for THC/CBD. Yes, we all know you should not vape oil under any circumstances as the risk of pneumonia is too high. But, according to some research, MCT is the exception to that rule and why these vendors are using it.

With that said, my concern becomes the reliability of the MCT producer; both for anyone wishing to make their own as well as the above mentioned vendors. If any long chains make it through the process, the risk is still there.

So whether you want to consider this route, or purchase a vape product containing MCT, be sure to do your own research and make an informed decision.

Back to the darkside
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Please do not "hesitate" on stuff like that. As far as Im concerned, the hazards are more important than anything,,,,and nobody thinks about all of them all of the time. On that note...Coconut oil is a MCT but they are using something more refined, no? Still, either way, good info!
 
Kicknitup1 said:
Please do not "hesitate" on stuff like that. As far as Im concerned, the hazards are more important than anything,,,,and nobody thinks about all of them all of the time. On that note...Coconut oil is a MCT but they are using something more refined, no? Still, either way, good info!
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MCT is a fractional distillation of coconut oil, but not all fractional distillations of coconut oil are MCT. And that's part of the problem. From the research I've done, I believe it may be safe to vape MCT oil, but that is my belief and only if I were sure out truly was MCT.

Trust me, pneumonia is not something to take lightly. I had it once, 50 years ago, and still remember it clearly. That alone should give anyone pause.

Back to the darkside
 
Kicknitup1 said:
Thanks Canyon. It is perhaps the water content that is grabbing terpenes because they are definitely soluble in water. Using 190 proof, maybe @ only 5% water, it's not much of a problem. Everyone is chilling the alcohol to (?) prevent it from absorbing the chlorophyll & such (?). So, to clarify that principle, is chilling to cut down on the alcohol picking up the undesirables OR is it to cut down on the water content picking up the undesirables????
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I think there is some widespread confusion about water solubility of terpenes and if you surf the web a bit that confusion becomes evident. This is a prime example of taking a stance on an issue and you can definitely find substantiating evidence.

TCI America, an international chemical company states:

"In general, most of the terpenes are insoluble in water but soluble in ethanol, chloroform and diethyl ether."

Steep Hill Labs says terpenes are widely considered nonpolar (not water soluble) but some of the larger, molecularly heavier terpenes can exhibit polar characteristics.

(Having to rely on memory here which sometimes isn't reliable) I think it was a reasearch paper on pub.net that classified terpenes as water soluble only under endothermic conditions; presence of heat and pressure, basically.

Dinafem, in their explanation of steam distillation of terpenes, avers without reservation that terpenes are water soluble. Their reasoning is that the "boiled off" terpenes travel up the distillation stack in conjunction with the steam and enter the condensation chamber simultaneously. They go on to explain that after condensation, the terpenes are easily reclaimed because they're floating on top of the water. If, in the end results, terpenes are found floating on top of water, should this be considered water soluble? Some that are more chemically inclined may be able to shed some light on this.

Now, on to why we chill ethanol. My mentor gave a twofold legitimacy to it.

One, we freeze the material for 24 hrs shaking vigorously a few times. Supposedly, this makes the trichomes very brittle and are easily separated from the plant matter. I've never made dry ice hash but I assume similar principles apply. If we introduced ethanol at a higher temp than that of the material, it would negate part of our chilling effort.

Secondly, at 0 degrees the water content of the ethanol loses much of its ability to absorb the polar elements of the material, i.e. chlorophyll, flavonoids, waxes, etc that can cause unpleasant taste in the final product.
 
"Secondly, at 0 degrees the water content of the ethanol loses much of its ability to absorb the polar elements of the material, i.e. chlorophyll, flavonoids, waxes, etc that can cause unpleasant taste in the final product. "

And unfortunately most of that bad stuff is also soluble in EVOO, et al. NOT as much as water by any means but still enough to make the oil taste like crap.

Hey, talking about taking better notes... I think I will print out the last several pages of our board. Take a red pen and write a keyword beside every paragraph I want to follow...ok, I love it all. I have learned so much about other parts of the puzzle from dirt to thc isolate that I wasn't even planning to learn (I can't grow here. End of story). But gaining understanding in those areas gave me insight into the things I was out to learn (See Title of This Forum).

Anyway, KeyWord what paragraphs are about like "Ethanol Extraction Properties" and then go back & update as info comes in.
 
Kicknitup1 said:
"Secondly, at 0 degrees the water content of the ethanol loses much of its ability to absorb the polar elements of the material, i.e. chlorophyll, flavonoids, waxes, etc that can cause unpleasant taste in the final product. "

And unfortunately most of that bad stuff is also soluble in EVOO, et al. NOT as much as water by any means but still enough to make the oil taste like crap.
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I know what you mean. My first attempt to do a direct extraction in coconut oil using my magic butter machine (now a really great doorstop), my edibles tasted so bad I through everything away.
 
Kicknitup1 said:
Throwing out some random observations related to this- CCO does not dissolve in 151 proof for crap. If you make it, you have probably overdone it with heat. Same with VG & PG. Now those, you can make happen but it's hard. Saw Ruffhouse do it with help from Cat Scientific. Even Cat had trouble. They finally made it happen by multiple heat & blend cycles....and a serious blender (homogenizer). ...Going back & forth here between ejuice & a stripper for general use here..... I resolved it by adding 1 ml of EVOO to give the CCO a better place to go. It worked but did take several blends. BUT 2 days later there was NO separation. I don't like it but that is a solution for edibles BUT NOT FOR VAPING! By the same token, lets just take a moment for a CAUTION[/

I hear people say all the time that you don't have to worry about Butane cause it evaporates at around 30f. True, but you will NOT get it all without a vacuum setup. I will let you decide if that is close enough. And, back to me adding EVOO...well ya can't smoke that!
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Kickn, I'm really surprised that you're experiencing problems reconstituting cco in ethanol. May I ask what method you're using to create the cco? When you first add the ethanol and stir a bit, do you get partial dissolution or none at all?
 
"Kickn, I'm really surprised that you're experiencing problems reconstituting cco in ethanol. May I ask what method you're using to create the cco? When you first add the ethanol and stir a bit, do you get partial dissolution or none at all? "

I will pay more attention but I would say the bulk of it is not dissolving...from memory it's an oil on the top. I only have 151 to work with. I will try to find some 190 when I go out of state.

Unfortunately I'm not making my own CCO. I have a 1 ton Harbor press for when that day comes. Still working on heat plates. And, the weed here would be expensive to make it from. I was playing with vape liquid, vg, pg. But also, I make edibles from CCO so I need to dissolve it in something water soluble for gummy bears. Lecithin, vg, Ethanol & pg all help in the combining with the gelatin. I will be back to buds & EVOO when the tcheck arrives. I still have things (extraction techniques) up in the air that I started way back before my Canyon visit.
 
Kicknitup1 said:
"Kickn, I'm really surprised that you're experiencing problems reconstituting cco in ethanol. May I ask what method you're using to create the cco? When you first add the ethanol and stir a bit, do you get partial dissolution or none at all? "

I will pay more attention but I would say the bulk of it is not dissolving...from memory it's an oil on the top. I only have 151 to work with. I will try to find some 190 when I go out of state.

Unfortunately I'm not making my own CCO. I have a 1 ton Harbor press for when that day comes. Still working on heat plates. And, the weed here would be expensive to make it from. I was playing with vape liquid, vg, pg. But also, I make edibles from CCO so I need to dissolve it in something water soluble for gummy bears. Lecithin, vg, Ethanol & pg all help in the combining with the gelatin. I will be back to buds & EVOO when the tcheck arrives. I still have things (extraction techniques) up in the air that I started way back before my Canyon visit.
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Kickin, not necessarily the most most affordable option, but if counting gas and time it might be worthwhile to check out x-f-b alcohol, it's available on Amazon for delivery to all states.

Cheers from the darkside
 
I was in hopes your problem was similar to an experience I occasionally run into but looks like it's probably not related.

FWIW, however, I'll throw this out. Let me preface by saying I'm pretty much a one trick pony. I've found my comfort zone with ethanol extraction and my experience with other methods is extremely limited. I'm not sure if any of this will be applicable, or even of interest, to others performing other extraction methods.

In my early learning process, I would do an ethanol extraction and try to reduce it to provide the potency I desired. In my humid environment, I'd get a lot of water separation and had no alternative but to do a complete evaporation, including water, and then adding back virgin ethanol to obtain the proper ratio. In my experience, when reconstituting my cco, if the ethanol didn't readily dissolve it, it's probably something I don't want in my tincture anyway.

Ethanol is extremely efficient in quickly extracting cannabinods (and hopefully terpenes). But since it's very hygroscopic, if it's allowed to stay in contact with the material for an extended period (longer than a couple of hours) it's going to start leaching out the moisture content as well. With that moisture is also going to come the polar elements of cannabis,i.e. waxes, chlorophyll and other nasties. When I do a complete evaporation, what I have left is not only the oil but also all the yuckies that I may have leached out. Looking at it, however, there's absolutely no visual indication that it's anything other than pure oil.

Now this is what I'm leading up to. When I reconstitute the cco it dissolves with little effort in probably less than a minute. If the moisture content of my material was too high or I let it soak too long in the ethanol, I'll have globules of a tar like substance either stuck intensely to my container and/or floating suspended in my alcohol. These globules are made up of primarily a wax that has been extracted from the plant matter. While the color seems almost identical to oil, the texture is much stiffer and stickier than any type of glue I've ever experienced. It's impervious to alcohol or water. Even with very hot water it requires a good deal of mechanical effort to remove it. Running my container through the dishwasher still often leaves traces of the residue.

Do you suppose........
 
Bucudinkydow said:
Now this is what I'm leading up to. When I reconstitute the cco it dissolves with little effort in probably less than a minute. If the moisture content of my material was too high or I let it soak too long in the ethanol, I'll have globules of a tar like substance either stuck intensely to my container and/or floating suspended in my alcohol. These globules are made up of primarily a wax that has been extracted from the plant matter. While the color seems almost identical to oil, the texture is much stiffer and stickier than any type of glue I've ever experienced. It's impervious to alcohol or water. Even with very hot water it requires a good deal of mechanical effort to remove it. Running my container through the dishwasher still often leaves traces of the residue.

Do you suppose........
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This black, tarry, yukky stuff is what I ended up with on my first (and only) try to reduce a tincture (aged over time). So apparently I heated off everything good and had only the waxes and other unwanted stuff left. My tinctures are brewed the old way, covered in vodka or Bicardi in a mason jar for at least a month in a dark, cool cabinet.

I forgot about one I started months ago in Vodka and only decanted it mid November 2017. I wonder if I evaporated this out naturally, in a gas oven with only the pilot light on (it's always on), would I get a passable CCO for capsules?
 
AKgramma said:
This black, tarry, yukky stuff is what I ended up with on my first (and only) try to reduce a tincture (aged over time). So apparently I heated off everything good and had only the waxes and other unwanted stuff left. My tinctures are brewed the old way, covered in vodka or Bicardi in a mason jar for at least a month in a dark, cool cabinet.

I forgot about one I started months ago in Vodka and only decanted it mid November 2017. I wonder if I evaporated this out naturally, in a gas oven with only the pilot light on (it's always on), would I get a passable CCO for capsules?
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Open flame, even from a pilot light, and evaporated ethanol are never a good combination. I wouldn't try it. Evaporation in a good open space with a small fan blowing over it will give you the same end results, just take a little longer. Depending on relative humidity you should be able to do the deed in 12-24 hours. A bathroom with an exhaust fan is a good place or the kitchen under the stove hood.

Yes, cco caps are still a definite option. Letting it set that long you've leached out everything that plant had to give, good and bad. Go ahead and do the initial evaporation and do a trial capsule. If you have a sensitive stomach you could possibly experience a little uneasiness. If you pass the test go ahead and cap the rest. If it proves to be intolerable reach out and we may be able to salvage it with a little effort.

Good luck
BCDD
 
Bucudinkydow said:
Open flame, even from a pilot light, and evaporated ethanol are never a good combination. I wouldn't try it. Evaporation in a good open space with a small fan blowing over it will give you the same end results, just take a little longer. Depending on relative humidity you should be able to do the deed in 12-24 hours. A bathroom with an exhaust fan is a good place or the kitchen under the stove hood.

Yes, cco caps are still a definite option. Letting it set that long you've leached out everything that plant had to give, good and bad. Go ahead and do the initial evaporation and do a trial capsule. If you have a sensitive stomach you could possibly experience a little uneasiness. If you pass the test go ahead and cap the rest. If it proves to be intolerable reach out and we may be able to salvage it with a little effort.

Good luck
BCDD
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You say on top of the stove under the fan, but the stove is a natural gas stove. Will that be safe?
 
Extract and cap update
These numbers and the logic should be checked.
I called Steep Hill about what they wanted for concentrate samples. They need 0.3g of concentrate or one cap of the oil. I will probably have a cap tested.

I scraped up what I could, renced the dish with Everclear and dried that. It is still not all in one place. My best guess would be just shy of 5 grams extracted. Mathematically it should be 6.7grams. The recovery ratio would be close to 75% if only CBDA, CBD, THCA and THC were extracted. The oil looks clean. I only used two soaks of about 5 minutes plus I renced the dregs with the last of 750ml of Everclear and squeezed it out all that I could with it so cold. There were no signs of chlorophyll. I think two 30 minute washes and a better last squeeze would bring the recovery up a lot without picking up much of the undesirables.

From the Thunderstruck 2 Decarb charts we have:
CBD 2.9%
CBDA 12.3%
THC 7%
THCA < 2%

I used 20 grams of raw dried and 9 grams of the #2 decarb.

These are the gross amounts I came up with for each material.
20 grams raw
CBDA @ 123mg per gram X 20g = 2,460mg
CBD @ 29mg/0.88 = 33mg of CBDA X 20g = 660mg
THC @ 70mg/0.88 = 79.5mg of THCA X 20 = 1,590mg
THCA < 2%

9 grams 2nd decarb
CBD @ 29mg X 9 = 261mg
CBDA @123mg X 9 = 1,107mg
THC @ 70mg X 9 = 630mg
THCA < 2%

These are the combined totals.
CBDA = 2,460 + 660 +1,107 = 4,227mg
CBD = 261mg
THCA = 1,590mg
THC = 630mg
Total 6,708mg

This converts to percent and mg/g
CBDA = 4,227/6,708 = 63% = 630mg/g
CBD = 261/6,708 = 3.89% = 38.9 mg/g
THCA = 1,590/6708 = 23.7% = 237 mg/g
THC = 630/6708 = 9.39% = 93.9 mg/g
Total cannabinoids= 999.8 mg/g = 99.98%

1ml of coconut oil weighs about 0.9g.
A 00 cap holds about 0.9ml.

CAPS @ 80g oil per gram of extract.
CBDA = 7.875mg/g, 7.875 X 0.90ml = 7.088 mg per cap
CBD = 0.486mg/g, 0.486 X 0.9ml = 0.437 mg per cap
THCA = 3.413mg/g, 3.413 X 0.90ml = 3.072 mg per cap
THC = 1.174mg/g, 1.174 X 0.90ml = 1.057 mg per cap
Total mg/g = 12.966mg/g, 12.966 X 0.90 (the density of the coconut oil) = 11.669 per cap
Total = 7.088 + 0.437 + 3.072 + 1.057 = 11.654 per cap

I never know, you know, best

 
i was suggesting using the hood for exhausting the fumes. If your cooktop is also gas please scratch that suggestion. Bare in mind, evaporating ethanol creates fumes equally as flammable as gasoline. Please take precautions and keep it away from any open flames. I generally use my outside workshop but a friend doesn't have access to outside facilities and uses his seldomly used guest bathroom with the exhaust fan running.
 
Re: My last post.
The caps are for my wife. The idea is to have 1mg of the and 10-12mg of other cannabiniods. Subtracting the THC from the cannabinoid total of a cap makes it 1.057mg per cap of THC to 10.597mg of other cannabinoids.

The CBD is lower than I would like. I want to test the oil without lecithin or adding any of the CBD based terpene profile concentrate. I will mix a small batch of 80 grams of coconut oil with 1 gram of concentrate and pull a sample for testing.

She has 20 or 30 of the 10mg CBD caps left. I will probably try having her drop the CBD caps for a while and just take the new batch for a while. They can be added back into the mix or some other quantity of CBD could be used.


 
Canyon, that looks like an awful lot of work. Thanx for sharing. My hats off to you for your mathematics skills!

I must have missed something back upstream. When did you get your terpene profile concentrate? Is it a blend to mimic a certain strain? What's your impression?

I'm anxiously expecting four different blends from True terpenes tomorrow. I have previously had a couple of individual isolates, limonene and a-pinene and was overwhelmed at how effective they were. I was expecting some over-hyped snake oil but was pleasantly surprised.

Please share your experience.
 
Bucudinkydow said:
Canyon, that looks like an awful lot of work. Thanx for sharing. My hats off to you for your mathematics skills!

I must have missed something back upstream. When did you get your terpene profile concentrate? Is it a blend to mimic a certain strain? What's your impression?

I'm anxiously expecting four different blends from True terpenes tomorrow. I have previously had a couple of individual isolates, limonene and a-pinene and was overwhelmed at how effective they were. I was expecting some over-hyped snake oil but was pleasantly surprised.

Please share your experience.
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I had to do most of it to figure out what ratio I needed for a blend that was about 1 to 10 THC to other cannabinoids. I hope I have it correct. I never know. BTW, add, subtract, multiply and divide is my limit.

A few months ago I bought a 1/4 gram of what is called strain specific CBD TerpSugar, xxx.terpsugar.com. They don't have a lot of products. There web site is bare bones. If you click on more options, you can select strains and find out that they offer 5 strains. Anyway, I bought it and a gram later on for about a $10 markup over there site prices from local a head shop.
I am not sure but I think they are taking a range of terpenes off of a strain and adding that to a CBD isolate. It would be interesting to find out how much they are actually putting in it. The cannabinoid listing is 99.49% CBD. The 3 strains I have flower terpene profiles on have 0.423%, 0.456% and 1.55% total terpene content.

I tried a medium sized nail hit and got somewhere between light headed and dizzy for about two minutes. Then, it faded into a calm feeling that was noticeable but not overly strong. After 20 minutes or so I did a bowl of high THC bud. That was a very pleasant high, calm and clear headed. I think I smoked the rest of it a little at a time by adding a little on top of a bowl of buds.

Half of the 1 gram batch was used to make 10ml 00 caps for my wife. She has been taking one at night for about three weeks now. That is about twice what she was getting dividing up commercial CBD chocolate bars. She is sleeping slightly better all though she is still mostly nocturnal.

I will switch her over to the new batch when I get them made up. If they show signs of helping with pain, restless leg syndrome or opiate withdrawal I will try adding the extra CBD back into what she is taking. With luck it will work out that way.

How did you use the limonene and a-pinene? What did you like about it?

Keep us posted.


 
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